CN103232609B - A kind of preparation method of flyash modified nano aluminium oxide/polyimide composite film - Google Patents
A kind of preparation method of flyash modified nano aluminium oxide/polyimide composite film Download PDFInfo
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- CN103232609B CN103232609B CN201310147343.6A CN201310147343A CN103232609B CN 103232609 B CN103232609 B CN 103232609B CN 201310147343 A CN201310147343 A CN 201310147343A CN 103232609 B CN103232609 B CN 103232609B
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Abstract
The invention discloses a kind of preparation method of flyash modified nano aluminium oxide/polyimide composite film.The method utilizes nano alumina sol to obtain the Kapton of nano aluminium oxide hydridization, obviously can improve corona-resistance property and the dielectric properties of Kapton, its Inverter fed motor life-span be the 8-9 of pure Kapton doubly; The present invention also utilizes the filling-modified Kapton of flyash, improves and overcome the defect of pure Kapton, can significantly improve its physical strength, hardness and wear resistance and heat decomposition temperature, thus improves its over-all properties.The new type polyimide nano compound film that the present invention prepares have high temperature resistant, mechanical property good, electric property is excellent, be easy to forming process, the features such as cost is low, meet completely aerospace, microelectronics, electrically, the requirement of the hi-tech development such as chemical industry, energy technology.
Description
Technical field
The present invention relates to a kind of preparation method of polyimide, be specifically related to a kind of preparation method of flyash modified nano aluminium oxide/polyimide composite film.
Background technology
Polyimide (PI) is the base polymer containing imide ring imide group on main chain, is obtained by diprotic acid and diamine polycondensation.Kapton is a kind of novel high temperature resistant organic polymer thin film, the film clasp Y insulation Y material that performance is best in the world at present, it salivates film forming through polycondensation by pyromellitic acid anhydride (PMDA) and diaminodiphenyl oxide (ODA) in extremely strong property solvent N,N-DIMETHYLACETAMIDE (DMAC), then forms through imidization.Because PI has superior thermal characteristics, electrical property, mechanical property and chemical stability, be widely used in the every field such as aerospace, spaceship, navigation, rocket-powered missile, automobile, electrical apparatus insulation, nuclear industry, satellite, nuclear-propelled submarine, microelectronics (comprising IC, printed circuit board etc.), liquid-crystal display, medical treatment, packaging precision optical machinery.China's Kapton production technology is more several years ago compared, that quality or output are all greatly improved and growth, but compared with advanced foreign technology product, larger gap is also there is in over-all properties, domestic Kapton also exists that poor product quality, over-all properties are unstable, product becomes more meticulous the shortcomings such as degree is inadequate, kind is few, have impact on its application.
Summary of the invention
The object of the invention is the preparation method providing a kind of flyash modified nano aluminium oxide/polyimide composite film, and the Kapton that the method prepares is high temperature resistant, mechanical property good and excellent insulation performance, thus improves its over-all properties.
The technical solution used in the present invention is as follows:
A preparation method for flyash modified nano aluminium oxide/polyimide composite film, comprises the following steps:
(1) process of raw material
Raw material pyromellitic acid anhydride (PMDA), 4 is taken by weight 1-1.5:0.8-1:25-30,4 '-diaminodiphenyl ether (ODA) and N, N-dimethyl second phthalein amine (DMAC), then respectively by PMDA dry 3-4 hour at 130-140 DEG C, ODA is dry 2-3 hour at 105-110 DEG C, solvent DMAC distills, and extracts 161-164 DEG C of cut;
(2) preparation of nano aluminium oxide/PAA solution
Take the ODA of certain mass, add the DMAC of 6/10-8/10 again, rock and add the nano alumina sol being equivalent to solution quality 15-20% after ODA dissolves completely, stir, then PMDA is divided equally trisection, every within 20-30 minute, to add a to above-mentioned solution in 0-5 DEG C of ice bath, fill nitrogen condition under stir 20-30 minute, to add after PMDA continuously stirring 5-6 hour again, obtain the nano aluminium oxide/PAA solution of thickness;
(3) flyash modified nano aluminium oxide/PAA solution
Get the flyash dry 2-3 hour at 110-120 DEG C being equivalent to nano alumina sol and PAA mixing solutions weight 3-5%, add and be equivalent to the Sodium hexametaphosphate 99 of flyash weight 2-3%, the γ-aminopropyl triethoxysilane of 0.5-1%, 2000-3000rpm high-speed stirring 10-15 minute, dry, pulverize porphyrize and cross 200-300 mesh sieve; Then added in remaining DMAC by the flyash after process, be 20-30KHz in frequency, power is ultrasonic disperse 15-20 minute under 400-600W condition, obtained flyash DMAC suspension; Finally mixed with nano aluminium oxide/PAA solution by flyash DMAC suspension, continuously stirring 6-8 hour uniformly solution, obtains flyash modified nano aluminium oxide/PAA solution;
(4) curtain coating
Get the triphenylphosphate that above-mentioned obtained flyash modified nano aluminium oxide/PAA solution adds 0.5-0.8%, stir, after placing 20-24 hour froth breaking, resin solution is slowly flow on smooth steel band by casting machine salivation mouth, and control its thickness at 0.08-0.01mm, the steel band scribbling resin solution is transported to dry 10-15 minute in the drying tunnel of 110-120 DEG C, forms one deck PAA film, after film cooling, it is peeled off from steel band;
(5) longitudinal stretching
PAA film after stripping is transported to longitudinal stretching machine and carries out longitudinal stretching, draw speed is 1-6m/min, working width 1200-1300mm, and stretch ratio is 1:1-1:3, and draft temperature is 80-180 DEG C;
(6) cross directional stretch
Film through longitudinal stretching machine is heated to 140-150 DEG C equably in transverse drawing mill, then under 2-15m/min speed, carries out cross directional stretch, working width inlet section: 900-1200mm, outlet section 1000-1400mm;
(7) imidization
Stretched film is carried out hot imidization 1-2 hour at 350-370 DEG C, is cooled to normal temperature and namely obtains Kapton through imidization;
(8) trimming rolling
On request trimming is carried out to Kapton, then with tractor, shaping Kapton is batched rolling, packaging warehouse-in.
The solid content of described nano alumina sol is 20-25%.
Beneficial effect of the present invention:
The present invention utilizes nano alumina sol to obtain the Kapton of nano aluminium oxide hydridization, obviously can improve corona-resistance property and the dielectric properties of Kapton, its Inverter fed motor life-span be the 8-9 of pure Kapton doubly; The present invention also utilizes the filling-modified Kapton of flyash, improves and overcome the defect of pure Kapton, can significantly improve its physical strength, hardness and wear resistance and heat decomposition temperature, thus improves its over-all properties.The new type polyimide nano compound film that the present invention prepares have high temperature resistant, mechanical property good, electric property is excellent, be easy to forming process, the features such as cost is low, meet completely aerospace, microelectronics, electrically, the requirement of the hi-tech development such as chemical industry, energy technology.
Embodiment
A preparation method for flyash modified nano aluminium oxide/polyimide composite film, comprises the following steps:
(1) process of raw material
Raw material pyromellitic acid anhydride (PMDA), 4 is taken by weight 1:1:30,4 '-diaminodiphenyl ether (ODA) and N, N-dimethyl second phthalein amine (DMAC), then respectively by PMDA at 140 DEG C dry 3 hours, ODA at 105 DEG C dry 3 hours, solvent DMAC distills, and extracts 161-164 DEG C of cut;
(2) preparation of nano aluminium oxide/PAA solution
Take the ODA of certain mass, add the DMAC of 6/10 again, rock and add the nano alumina sol (solid content is 25%) being equivalent to solution quality 16% after ODA dissolves completely, stir, then PMDA is divided equally trisection, every within 30 minutes, to add a to above-mentioned solution in 2 DEG C of ice baths, fill nitrogen condition under stir 30 minutes, to add after PMDA again continuously stirring 6 hours, obtain the nano aluminium oxide/PAA solution of thickness;
(4) flyash modified nano aluminium oxide/PAA solution
Get the flyash at 110 DEG C dry 3 hours being equivalent to nano alumina sol and PAA mixing solutions weight 5%, add and be equivalent to the Sodium hexametaphosphate 99 of flyash weight 2.5%, the γ-aminopropyl triethoxysilane of 0.8%, 3000rpm high-speed stirring 10 minutes, dry, pulverize porphyrize and cross 300 mesh sieves; Then being added in remaining DMAC by the flyash after process, is 25KHz in frequency, and power is ultrasonic disperse 15 minutes under 500W condition, obtained flyash DMAC suspension; Finally mixed with nano aluminium oxide/PAA solution by flyash DMAC suspension, continuously stirring 6 hours uniformly solution, obtains flyash modified nano aluminium oxide/PAA solution;
(4) curtain coating
Get the triphenylphosphate that above-mentioned obtained flyash modified nano aluminium oxide/PAA solution adds 0.5-0.8%, stir, after placing 20-24 hour froth breaking, resin solution is slowly flow on smooth steel band by casting machine salivation mouth, and control its thickness at 0.08-0.01mm, the steel band scribbling resin solution is transported to dry 10-15 minute in the drying tunnel of 110-120 DEG C, forms one deck PAA film, after film cooling, it is peeled off from steel band;
(5) longitudinal stretching
PAA film after stripping is transported to longitudinal stretching machine and carries out longitudinal stretching, draw speed is 3m/min, working width 1200mm, and stretch ratio is 1:2, and draft temperature is 120 DEG C;
(6) cross directional stretch
Film through longitudinal stretching machine is heated to 145 DEG C equably in transverse drawing mill, then under 8m/min speed, carries out cross directional stretch, working width inlet section: 1000mm, outlet section 1300mm;
(7) imidization
Stretched film is carried out hot imidization 2 hours at 350 DEG C, is cooled to normal temperature and namely obtains Kapton through imidization;
(8) trimming rolling
On request trimming is carried out to Kapton, then with tractor, shaping Kapton is batched rolling, packaging warehouse-in.
The Kapton service check that the present embodiment prepares is as following table:
| Project | Detected result |
| Tensile strength (MPa) | 105.3 |
| Breaking tenacity (kg/m 2) | 21.6 |
| Elongation at break (%) | 52.8 |
| Dielectric strength (kv/mm) | 186.9 |
| Volume resistance (Ω cm) | 3.2×10 16 |
Claims (2)
1. the preparation method of flyash modified nano aluminium oxide/polyimide composite film, it is characterized in that comprising the following steps: the process of (1) raw material takes raw material pyromellitic acid anhydride (PMDA), 4 by weight 1-1.5:0.8-1:25-30,4 '-diaminodiphenyl oxide (ODA) and N, N-N,N-DIMETHYLACETAMIDE (DMAC), then respectively by PMDA dry 3-4 hour at 130-140 DEG C, ODA is dry 2-3 hour at 105-110 DEG C, solvent DMAC distills, and extracts 161-164 DEG C of cut; (2) preparation of nano aluminium oxide/PAA solution takes the ODA of certain mass, add the DMAC of 6/10-8/10 again, rock and add the nano alumina sol being equivalent to solution quality 15-20% after ODA dissolves completely, stir, then PMDA is divided equally trisection, every within 20-30 minute, to add a to above-mentioned solution in 0-5 DEG C of ice bath, fill nitrogen condition under stir 20-30 minute, to add after PMDA continuously stirring 5-6 hour again, obtain the nano aluminium oxide/PAA solution of thickness; (3) flyash modified nano aluminium oxide/PAA solution gets the flyash dry 2-3 hour at 110-120 DEG C being equivalent to nano alumina sol and PAA mixing solutions weight 3-5%, add and be equivalent to the Sodium hexametaphosphate 99 of flyash weight 2-3%, the γ-aminopropyl triethoxysilane of 0.5-1%, 2000-3000rpm high-speed stirring 10-15 minute, dry, pulverize porphyrize and cross 200-300 mesh sieve; Then added in remaining DMAC by the flyash after process, be 20-30KHz in frequency, power is ultrasonic disperse 15-20 minute under 400-600W condition, obtained flyash DMAC suspension; Finally mixed with nano aluminium oxide/PAA solution by flyash DMAC suspension, continuously stirring 6-8 hour uniformly solution, obtains flyash modified nano aluminium oxide/PAA solution; (4) curtain coating gets the triphenylphosphate that above-mentioned obtained flyash modified nano aluminium oxide/PAA solution adds 0.5-0.8%, stir, after placing 20-24 hour froth breaking, resin solution is slowly flow on smooth steel band by casting machine salivation mouth, and control its thickness at 0.08-0.01mm, the steel band scribbling resin solution is transported to dry 10-15 minute in the drying tunnel of 110-120 DEG C, forms one deck PAA film, after film cooling, it is peeled off from steel band; (5) the PAA film after peeling off is transported to longitudinal stretching machine and carries out longitudinal stretching by longitudinal stretching, and draw speed is 1-6m/min, working width 1200-1300mm, and stretch ratio is 1:1-1:3, and draft temperature is 80-180 DEG C; (6) cross directional stretch is heated to 140-150 DEG C through the film of longitudinal stretching machine equably in transverse drawing mill, then under 2-15m/min speed, carries out cross directional stretch, working width inlet section: 900-1200mm, outlet section 1000-1400mm; (7) stretched film is carried out hot imidization 1-2 hour by imidization at 350-370 DEG C, is cooled to normal temperature and namely obtains Kapton through imidization; (8) trimming rolling carries out trimming to Kapton on request, then with tractor, shaping Kapton is batched rolling, packaging warehouse-in.
2. the preparation method of a kind of flyash modified nano aluminium oxide/polyimide composite film according to claim 1, is characterized in that, the solid content of described nano alumina sol is 20-25%.
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| CN103739205B (en) * | 2013-11-08 | 2017-06-13 | 北京京东方光电科技有限公司 | Functional material and preparation method thereof, display structure form material, color membrane substrates, display device |
| EP3176225B1 (en) | 2014-07-29 | 2020-02-19 | Boe Technology Group Co. Ltd. | Functional material, preparation method therefor, organic light-emitting diode display panel |
| WO2016015409A1 (en) | 2014-07-29 | 2016-02-04 | 京东方科技集团股份有限公司 | Functional material, preparation method therefor, alignment material, liquid crystal display substrate |
| CN104191633B (en) * | 2014-08-27 | 2017-02-15 | 桂林电器科学研究院有限公司 | Cold processing process and polyimide film production line for manufacturing polyimide film |
| CN104191635B (en) * | 2014-09-19 | 2017-02-15 | 桂林电器科学研究院有限公司 | Method for improving physical properties of polyimide film and polyimide film production line |
| CN105732005B (en) * | 2016-01-20 | 2018-05-01 | 南京理工大学 | A kind of flexibility perovskite heat controlled thin film and preparation method thereof |
| CN106497051A (en) * | 2016-10-07 | 2017-03-15 | 常州市鼎升环保科技有限公司 | A kind of preparation method of polyimide-based Inverter fed motor material |
| CN107501549A (en) * | 2017-06-22 | 2017-12-22 | 莱芜中天绝缘材料有限公司 | A kind of preparation method of nano aluminium oxide doped polyimide film |
| CN112280036A (en) * | 2020-11-17 | 2021-01-29 | 潍坊弘润新材料有限公司 | Processing technology of polyimide film |
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